CN102002343A - Heat-storage and heat-preservation microcapsules and preparation method and application thereof - Google Patents
Heat-storage and heat-preservation microcapsules and preparation method and application thereof Download PDFInfo
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- CN102002343A CN102002343A CN2010105144152A CN201010514415A CN102002343A CN 102002343 A CN102002343 A CN 102002343A CN 2010105144152 A CN2010105144152 A CN 2010105144152A CN 201010514415 A CN201010514415 A CN 201010514415A CN 102002343 A CN102002343 A CN 102002343A
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Abstract
The invention relates to phase-change energy-storage microcapsules and a preparation method and application thereof, in particular to heat-storage and heat-preservation microcapsules by taking a core material as a phase-change energy-storage material, and a preparation method and application thereof. Each microcapsule consists of a core, an internal nuclear shell and an external nuclear shell, wherein the core material is an organic phase-change material; the internal nuclear shell takes vinyl monomers as polymerizing monomers and packs the core through interfacial polymerization; and the external nuclear shell takes etherified melamine resin prepolymers as polymerizing monomers and packs the internal nuclear shell through in-situ polymerization. The heat-storage and heat-preservation microcapsules have thermosetting properties of microcapsule walls, high processing resistance, high abrasive resistance and high durability. The heat-storage and heat-preservation microcapsules can be used for heat-preservation finishing of textiles and building heat-preservation materials and can ensure the higher phase change energy of the organic phase-change materials of the cores of the heat-storage and heat-preservation microcapsules, the organic phase-change materials cannot flow or shift after phase change, so that a temperature control function can be enduringly kept.
Description
Technical field
The present invention relates to a kind of microcapsules of storing energy through phase change and its production and application, relating in particular to a kind of core material of examining is heat storing and heat preserving microcapsule of phase-changing energy storage material and its production and application.
Background technology
Phase-changing energy storage material is to improve capacity usage ratio, and can endergonic adaptively intelligent material.Aspect building inner decorative material, phase change material can make full use of environmental energy, obtains effect cool in summer and warm in winter.Aspect textiles, the textiles of traditional natural fiber (as cotton, fiber crops, silk, hair) and man-made fiber (as terylene, nylon, acrylic fibers and regenerated fiber etc.) has certain thermal resistance that heat scatters and disappears that prevents, its insulated capacity is to have the amount of the still air that comprises in the textiles to determine.
And phase change material can be in envrionment temperature by being lower than the heat in the absorbing environmental when being higher than transformation temperature, solid-liquid takes place to be changed mutually, until phase change material is liquid by solid state transformation all, and when envrionment temperature is lower than transformation temperature again, phase change material can be emitted the heat of absorption again, the generation liquid-solid phase changes, and this heat absorption can make material temperature keep relative constant within a certain period of time with the heat release function.
The research of thermal storage and energy accumulation material and Material Used aspect thereof has had certain progress, and wherein the research about phase-change microcapsule also just starts to walk.Most of phase-change microcapsules promptly enable to guarantee to have big phase-change energy, but after undergoing phase transition, can take place to flow and migration, and make the temperature controlled function lose, and the phase change material that runs off will react with environment and the external sight of ectocrine, patent 200710047217.8 adopts methods such as porous material loadingization or vacuum impregnation, but its materials ' durability of making can be poor, can undergo phase transition material transition, loss, as coating, can cause the corrosion of construction substrate.
Patent 200510024707.7 and patent 200810068422.7 also attempt having adopted synthesizing microcapsules of storing energy through phase change by using method of emulsion polymerization.But its microcapsule shell wear resistance and weather resistance all have been difficult to breakthrough, phase change material inside takes place easily leak, and textiles overall performances such as oil mark, feel occur and change greatly on textiles.
Summary of the invention
The technical problem to be solved in the present invention is: a kind of shell wear resistance and good endurance are provided, are difficult for heat storing and heat preserving microcapsule that take place the phase change material inside leakage and its production and application.
The technical solution adopted for the present invention to solve the technical problems is: a kind of heat storing and heat preserving microcapsule, and it is made up of nuclear core, internal layer nucleocapsid and outer nucleocapsid, and the nuclear core material is an organic phase change material; The internal layer nucleocapsid is polymerization single polymerization monomer with the vinyl monomer, by interfacial polymerization parcel nuclear core; Outer nucleocapsid is a polymerization single polymerization monomer with the etherification melamine resin performed polymer, by in-situ polymerization wrapping inner layer nucleocapsid.These heat storing and heat preserving microcapsule are a kind of ball-type capsule, and capsule wall has thermoset nature, and anti-processing characteristics is better.
Consider the phase point temperature of suitable environment and material, described nuclear core material is that carbonatoms is 15~50 straight-chain paraffin, refined wax and semi-refined paraffin wax one or more a mixture wherein.
When selecting the nucleocapsid monomer, consider microcapsule shell compactness and with the reactivity of blend, described vinyl monomer structure is one or more the mixture in following structure (1) and (2);
Structure (1) is:
Wherein, R1 is H, CH
3Perhaps C
2H
5, R2 is phenyl, substituted-phenyl, C1, CN, alkyl oxide or OCOCH
3
Structure (2) is:
Wherein, R1 is H, CH
3Perhaps C
2H
5, X is the aliphatic chain of the C1~C8 of the aliphatic chain of C1~C8 or hydroxyl;
Described etherification melamine resin performed polymer is the etherificate body of following structure (3) or structure (4):
Structure (3) is:
Structure (4) is:
Therein ethylene base monomer and etherification melamine resin performed polymer consumption are 100%~1000% of nuclear core material quality; Therein ethylene base monomer is 5~25% of an etherificate melmac quality; Initiator is ammonium persulphate or Potassium Persulphate.
The preparation method of aforesaid heat storing and heat preserving microcapsule has following processing step:
A, the above temperature of selection nuclear core material fusing point, in high shearing mixing emulsor high speed homogenizing, the speed of high speed homogenizing is 10000~12000rpm with organic phase change material, dispersion emulsifier and distilled water;
B, stirring are warming up to 75~80 ℃ and add initiators and vinyl monomer, the wall building of polymerization internal layer nucleocapsid;
C, be cooled to room temperature, regulate pH to 2~5, under agitation condition, drip etherification melamine resin, be warming up to 55~65 ℃ of insulation 1~2h and carry out outer nucleocapsid wall building;
D, cooling, ammoniacal liquor is neutralized to pH=7, discharging.
As preferably, the HLB value of described dispersion emulsifier is 11~15, is any or several arbitrary combination in polymer dielectric tensio-active agent, nonionogenic tenside and the aniorfic surfactant.
For improving the wear resistance and the weather resistance of microcapsule wall, the wall building of described internal layer nucleocapsid is the vinyl monomer secondary or the above repetition of the secondary wall building of different amounts.
Be wear resistance and the weather resistance that further improves microcapsule wall, described outer nucleocapsid wall building is the etherification melamine resin secondary or the above repetition of the secondary wall building of different amounts.
Aforesaid heat storing and heat preserving microcapsule are as the application of textiles heat preserving finishing, employing is padded, dipping, stamp, coating or spray pattern act on the heat storing and heat preserving microcapsule on the textiles, textiles comprises the fabric that various synthon, regenerated fiber, cotton, hair, silk or fiber crops are made, or their BLENDED FABRIC.
Aforesaid heat storing and heat preserving microcapsule are used as building thermal insulation material, the heat storing and heat preserving microcapsule are mixed in water-borne coatings or the putty, perhaps make indoor and outdoor body of wall thermostat layer with cement, mortar, lime, gypsum, slag, mineral wool, fiber-like, building sand or concrete.
The invention has the beneficial effects as follows, heat storing and heat preserving microcapsule of the present invention, capsule wall has thermoset nature, and anti-processing characteristics is better, wear resistance and good endurance.Can adopt pad, dipping, stamp, coating, spray pattern act on the textiles, be used for the textiles heat preserving finishing, need not to add tackiness agent, in the textiles use after the arrangement, phase change material inside can not take place leak, so that occur the overall performance variation of textiless such as oil mark, feel on textiles; Heat storing and heat preserving microcapsule of the present invention can be used for building thermal insulation material, it is mixed in water-borne coatings or the putty, perhaps make indoor and outdoor body of wall thermostat layer with cement, mortar, lime, gypsum, slag, mineral wool, fiber-like, building sand or concrete, it can guarantee that the organic phase change material of the nuclear core of heat storing and heat preserving microcapsule has big phase-change energy, and organic phase change material can not take place to flow after undergoing phase transition and migration, thereby can keep the temperature controlled function enduringly.
Embodiment
To help to understand the present invention by following examples, but not limit content of the present invention.Especially the data among the embodiment do not limit the consumption of each composition in the invention.
Embodiment 1
Under 40 ℃ with 200 parts in 50 parts of No. 30 paraffin, 2 parts of sorbester p17s, 3 parts of tween 80s, distilled water in high speed shear Mixingemulsificationmachine high speed homogenizing, homogenizing speed is 10000rpm, after 30 minutes, pour the emulsion of homogenizing into there-necked flask, put into constant temperature water bath, under agitation condition, be warming up to 80 ℃ of ammonium persulphate and 20 parts of methyl acrylates that add 0.5 part and carry out the internal layer wall building.After the cooling, regulating pH with acetic acid is 2~4, and stirring velocity is under the 300rpm, drip 80 parts etherification melamine resin, be warming up to 55 ℃, insulation 1~2h carries out outer wall building cooling, ammoniacal liquor is neutralized to pH=7, obtains the heat storing and heat preserving microcapsule solution, and spraying drying gets powdery heat storing and heat preserving microcapsule No. 1.
Embodiment 2
Pure knitted fabrics carries out heat storing heat preserving finishing:
Technology: adopt and pad mode: pad (two soak two rolls liquid carry over 70%) → dry (90~100 ℃) 2min
The padding liquid prescription:
No. 1 50g/L of heat storing and heat preserving microcapsule
The super gentle tackiness agent 30g/L of no aldehyde
The color of the cotton textiles before and after arrangement is basic identical, several no changes of feel, and formaldehyde content is 6.7mg/kg, and knitted fabrics is after washing 20 times, and through the insulation instrument test, clo value only reduces by 0.3.
Embodiment 3
Under 55 ℃ with 10 parts of No. 52 paraffin, 40 parts of No. 30 paraffin, 6 parts of Sodium Lauryl Sulphate BP/USPs, 4 parts of tween 80s, 300 parts of distilled water are in high speed shear Mixingemulsificationmachine high speed homogenizing, homogenizing speed is 10000rpm, after 30 minutes, pour the emulsion of homogenizing into there-necked flask then, put into constant temperature water bath, under agitation condition, be warming up to 80 ℃ of Potassium Persulphate and 22 parts of Jia Jibingxisuanyizhis that add 0.5 part and carry out the internal layer wall building, after the cooling, with the lemon acid for adjusting pH is 3~4,, stirring velocity is under the 300rpm, drips 80 parts etherification melamine resin, be warming up to 55 ℃, insulation 1~2h carries out outer individual layer wall building; After system is cooled to room temperature, drip 80 parts of etherification melamine resin once more under agitation condition, be warming up to 65 ℃, the skin wall building second time is carried out in insulation.Cooling, ammoniacal liquor is neutralized to pH=7, obtains the heat storing and heat preserving microcapsule solution, and spraying drying gets powdery heat storing and heat preserving microcapsule No. 2.
Embodiment 4
The textile printing heat preserving finishing
Directly the heat storing and heat preserving microcapsule are added in the paint-printing colour size, press pigment printing technology stamp then.
5 parts of coating
3 parts of thickening materials
4 parts of heat storing and heat preserving microcapsule
10 parts in the super gentle tackiness agent of no aldehyde
Add water to 100 parts
Technical process: bleached cotton fabric----stamp----preliminary drying (100 ℃ * 5min)----tentering (130 ℃ * 2min)
Embodiment 6
The polyamide fibre woven fabrics carries out the coating heat preserving finishing
Base cloth is the polyamide fibre woven fabrics, and coating-forming agent is 5% heat storing and heat preserving capsule dispersant liquid and 95% acrylic ester emulsion mixed solution, is thickened to required viscosity with ammoniacal liquor then, reaches more than 1000 centipoises.Use suspension scraper blade coating to polyamide fabric above coating-forming agent, thickness by floating cutter control coating, the coating amount is 20g/m2 (butt), then the fabric after the coating is sent in the loft drier, under 100~110 ℃ temperature, dry, bake at 140~150 ℃ again and can make mint flavored coated fabric in 2 minutes.
Embodiment 7
Under 55 ℃ with 35 parts of No. 20 paraffin, 15 parts of No. 52 paraffin, TX-47 part, 3 parts of tween 80s, 350 parts of distilled water are in high speed shear Mixingemulsificationmachine high speed homogenizing, homogenizing speed is 10000rpm, after 30 minutes, pour the emulsion of homogenizing into there-necked flask then, put into constant temperature water bath, under agitation condition, be warming up to 78 ℃ and add 0.4 part of Potassium Persulphate, 8 parts of vinylbenzene and butyl acrylate mixture are carried out the internal layer wall building for 10 parts, after the cooling, regulating pH with acetic acid is 3~4, stirring velocity is under the 300rpm, drip 67 parts etherification melamine resin, be warming up to 55 ℃, insulation 1~2h carries out outer individual layer wall building; After system is cooled to room temperature, drip 78 parts of etherification melamine resin once more under agitation condition, be warming up to 65 ℃, the skin wall building second time is carried out in insulation.Cooling, ammoniacal liquor is neutralized to pH=7, obtains the heat storing and heat preserving microcapsule solution, and spraying drying gets powdery heat storing and heat preserving microcapsule No. 3.
Embodiment 8
The building thermal-insulating coating prescription
Get the heat storing and heat preserving microcapsule No. 3, with No. 3, heat storing and heat preserving microcapsule: pure-acrylic emulsion: benzene emulsion: water=3: 4: 1: 5 (mass ratioes) mix, in the high speed shear Mixingemulsificationmachine, shear 30min, get homodisperse thermal insulation coatings with the 10000rpm velocity of shear.
Claims (9)
1. heat storing and heat preserving microcapsule is characterized in that: these microcapsule are made up of nuclear core, internal layer nucleocapsid and outer nucleocapsid, and the nuclear core material is an organic phase change material; The internal layer nucleocapsid is polymerization single polymerization monomer with the vinyl monomer, by interfacial polymerization parcel nuclear core; Outer nucleocapsid is a polymerization single polymerization monomer with the etherification melamine resin performed polymer, by in-situ polymerization wrapping inner layer nucleocapsid.
2. heat storing and heat preserving microcapsule as claimed in claim 1 is characterized in that: described nuclear core material is that carbonatoms is one or more the mixture in 15~50 straight-chain paraffin, refined wax and the semi-refined paraffin wax.
3. heat storing and heat preserving microcapsule as claimed in claim 1 is characterized in that: described vinyl monomer structure is one or more the mixture in following structure (1) and (2);
Structure (1) is:
Wherein, R1 is H, CH
3Perhaps C
2H
5, R2 is phenyl, substituted-phenyl, C1, CN, alkyl oxide or OCOCH
3
Structure (2) is:
Wherein, R1 is H, CH
3Perhaps C
2H
5, X is the aliphatic chain of the C1~C8 of the aliphatic chain of C1~C8 or hydroxyl;
Described etherification melamine resin performed polymer is the etherificate body of following structure (3) or structure (4):
Structure (3) is:
Structure (4) is:
Therein ethylene base monomer and etherification melamine resin performed polymer consumption are 100%~1000% of nuclear core material quality; Therein ethylene base monomer is 5~25% of an etherificate melmac quality; Initiator is ammonium persulphate or Potassium Persulphate.
4. as the preparation method of each described heat storing and heat preserving microcapsule of claim 1~3, it is characterized in that having following processing step:
A, the above temperature of selection nuclear core material fusing point, in high shearing mixing emulsor high speed homogenizing, the speed of high speed homogenizing is 10000~12000rpm with organic phase change material, dispersion emulsifier and distilled water;
B, stirring are warming up to 75~80 ℃ and add initiators and vinyl monomer, the wall building of polymerization internal layer nucleocapsid;
C, be cooled to room temperature, regulate pH to 2~5, under agitation condition, drip etherification melamine resin, be warming up to 55~65 ℃ of insulation 1~2h and carry out outer nucleocapsid wall building;
D, cooling, ammoniacal liquor is neutralized to pH=7, discharging.
5. the preparation method of heat storing and heat preserving microcapsule as claimed in claim 4, it is characterized in that: the HLB value of described dispersion emulsifier is 11~15, is any or several arbitrary combination in polymer dielectric tensio-active agent, nonionogenic tenside and the aniorfic surfactant.
6. the preparation method of heat storing and heat preserving microcapsule as claimed in claim 4 is characterized in that: the wall building of described internal layer nucleocapsid is the vinyl monomer secondary or the above repetition of the secondary wall building of different amounts.
7. the preparation method of heat storing and heat preserving microcapsule as claimed in claim 4 is characterized in that: described outer nucleocapsid wall building is the etherification melamine resin secondary or the above repetition of the secondary wall building of different amounts.
8. as of the application of each described heat storing and heat preserving microcapsule of claim 1~3 as the textiles heat preserving finishing, it is characterized in that: adopt pad, dipping, stamp, coating or spray pattern act on the heat storing and heat preserving microcapsule on the textiles, textiles comprises the fabric that various synthon, regenerated fiber, cotton, hair, silk or fiber crops are made, or their BLENDED FABRIC.
9. use as building thermal insulation material as each described heat storing and heat preserving microcapsule of claim 1~3, it is characterized in that: described heat storing and heat preserving microcapsule are mixed in water-borne coatings or the putty, perhaps make indoor and outdoor body of wall thermostat layer with cement, mortar, lime, gypsum, slag, mineral wool, fiber-like, building sand or concrete.
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Effective date of registration: 20171117 Address after: Daitou town of Liyang City Ferry Street 213311 Jiangsu city of Changzhou province 8-2 No. 7 Patentee after: Liyang Chang Technology Transfer Center Co., Ltd. Address before: No. 1, Wujin District, Changzhou, Jiangsu, Jiangsu Patentee before: Changzhou University |